Yarn



United States Patent US. Cl. 252-8.75 4 Claims ABSTRACT OF THE DISCLOSURE A polyamide or polyester textile yarn lubricating composition comprising a glyceryl triester, a sulfated glyceryl triester, a salt of a partial phosphate ester and a salt of a higher fatty acid. This composition is particularly useful for imparting exceptionally high level drawing characteristics to the polyamides or polyesters.

This application is a continuation-in-part of my application Ser. No. 485,926, filed Sept. 8, 1965 now abandoned.

This invention relates to lubricating compositions for continuous-filament synthetic yarns.

During the manufacture of synthetic continuous filament yarns, the yarns are repeatedly subjected to mechanical stresses by high-speed equipment. Consequently, it is common practice to provide the filamentary material with a conditioning agent which will serve to lubricate the yarn and retard the accumulation of static charges. The conditioning agents heretofore employed are not satisfactory when used to lubricate yarns which are to be textured in a heated environment since they undergo thermal decomposition, provide inadequate bulk, or contribute to yarn strength loss. 7

Accordingly, it it an object of this invention to provide an improved lubricating composition to be used in the manufacture of synthetic filaments.

It is a further object to provide an improved yarn bearing a lubricating composition amenable to high temperature processing and which will provide a uniform textured yarn with high bulk and low strength loss, and to provide a process for preparing that yarn.

Other objects of this invention will be apparent from the following detailed description.

These and other objects are accomplished in the present invention with a lubricating composition which consists essentially of a glyceryl triester, a sulfated glyceryl triester, a salt of a partial phosphate ester and a salt of a higher fatty acid. This composition is applied to filaments of a yarn either as a spin finish or at a later stage of processing, whereupon the yarn can be subjected to high temperatures and employed to provide uniform texturing and high bulk without sacrifice in the strength of the yarn. v j

The glyceryl triester used in this invention is an ester of glycerol and one or more aliphatic acids. The triester may be a natural or synthetic material and is preferably of a high level of purity as contaminants tend to decrease thermal stability. The triester should be stable to temperatures of at least 150 C. and not cause obnoxious fumes or smoke. The glyceryl triester may be formed from fatty acids'and preferably from saturated fatty acids having at least 12 to about 20 carbon atoms per molecule. Suitable glyceryl triesters include vegetable oils such as coconut oil, peanut oil, corn oil and synthetic esters such as glyceryl trilaurate, glyceryl tripalmitate, glyceryl, dilaurate-palmitate and the like. A preferred triester is refined coconut oil.

The sulfated glyceryl triester employed in the composition is a neutralized reaction product of sulfuric acid with a glyceryl triester containing aliphatic unsaturation and/or a hydroxyl group. Suitable glyceryl triesters which may be sulfated are those formed from one or more unsaturated fatty acids such as oleic acid, linoleic acid, and the like. A suitable hydroxyl-containing fatty acid is ricinoleic acid. Preferred materials are sulfated glyceryl trioleate, sulfated peanut oil, and sulfated olive oil. The sulfated fatty esters are neutralized with a suitable base and used in the form of their salts which is preferably an alkali metal salt, e.g., a sodium salt.

The salt of a partial phosphate ester used in this invention is obtained by neutralizing a partial ester obtained by reacting phosphorus pentoxide with a long chain aliphatic alcohol or mixture of such alcohols. The partial ester may be neutralized prior to or during the blending of the various ingredients to produce the composition. The number of carbon atoms in the alcohol is at least 6, e.g., 6 to 18, and preferably about 6 to 12. The alcohol may contain a branched chain. Alcohols that may be used to prepare the partial ester are, for example, n-octanol, ndecanol, 2-ethylhexanol, lauryl alcohol and the like. The partial ester may be the monoester or the diester or a mixture of the two so that there will be on the average of about 1 to 2, preferably 1.5 to 2, alcohol radicals per phosphorus atom. The partial alkyl ester is neutralized with the appropriate amount of an organic or inorganic base such as, for example, sodium hydroxide, potassium hydroxide, ammonia, triethanolamine and morpholine. A preferred material is the potassium salt of a mixture of monoand di-n-octyl phosphate.

The salt of a higher fatty acid used in an alkali metal, or amine salt of a fatty acid having at least 12 carbon atoms and preferably 12 to 18 carbon atoms per molecule. Among the suitable salts are potassium oleate, ammonium oleate, diethanolamine oleate and triethanolamine oleate. Mixtures of such salts are desirable ingredients, and a mixture of about equal amounts of potassium and triethanolamine oleates is a preferred material.

In preparing the compositions of this invention, the amounts of the ingredients are selected so as to provide the desired lubricating, antistatic and emulsifying properties. As will be described more fully hereinafter, a particular consideration is the selection of relative quantities to provide frictional characteristics commensurate with both good drawing and twist removal performances. The proportions of the ingredients are advantageously within the following ranges, expressed as parts by weight: glyceryl triester, about 5 to 50 parts, preferably 15 to 35 parts; sulfated glyceryl triester, about 20 to 50 parts, preferably 30 to 40 parts; phosphate ester salt, about 10 to 30 parts, preferably 15 to 25 parts; fatty acid salt, about 10 to 35 parts, preferably 15 to 30 parts. The composition can be prepared by blending together the glyceryl triester, sulfated glyceryl triester and a portion of the fatty acid salt and emulsifying the blend in water. The remainder of the fatty acid salt is mixed with the phosphate ester salt and the mixture emulsified in water. The two emulsions are then combined to form the final composition. Alternatively, a single oil base may be prepared by appropriate blending and the blend emulsified as desired,

In addition to the essential ingredients, small amounts of other materials may be added to the composition. For example, bactericide buffering agents, tints, antioxidants, and the like can be employed as circumstances may require.

These compositions are preferably used in the form of an aqueous emulsion in which the solids content is from about 5 to 30%, preferably about 10 to 20% by weight, based on the total weight of the emulsion. Application to the yarn can be made by passing the yarn across the face of a rotating roll partially emersed in the emulsion. The concentration and the roll speed are such as to apply to the yarn about 0.1% to 1.5% solids, preferably about '0.40 to 0.8% solids, by weight, based on the weight of the treated yarn. The emulsion is preferably applied to the yarn prior to drawing and most conveniently as the yarn emerges from the spinning cabinet. The emulsion may, however, be used as an overlay finish, i.e., applied over a previous coating, or it may be applied to a yarn from which a previously applied coating has been removed.

In practice of this invention the yarns employed are of nylon or polyester polymers. Typical nylons include polyhexamethylene adipamide, polycaproamide, the reaction product of dodecane dioic acid and bis-(p-aminocyclohexyDmethane or their amide forming derivatives, melt-blend nylons such as those described in British Patent 918,637 or other nylon or copolymer thereof. Any of the usual polyesters can be used with polyethylene terephthalates being preferred. All such materials are Well known and are described in the patent literature to which reference can be made. The filaments and yarns are of the usual denier for textile applications and can be of any of the many cross-sectional configurations now conventional in the art.

The compositions of this invention are particularly useful; for example, they provide an exceptionally high level of drawing performance. In one run wherein about 15,000 pounds of drawn polyamide yarn were produced, the breaks/lb. and percent filament wraps were 0.007 and 1.5% respectively. As is known to those skilled in this art, breaks/lb. of 0.01 and percent wraps of 5.0% are accepted standards of performance. The utilization of the compositions to lubricate the yarns in a drawing process is a preferred embodiment. In formulating the composition for drawing, the relative amounts of the individual ingredients should be selected so that the tension level of the yarn just prior to the draw pin is on the order of about to 25 grams. In general, this tension level is increased by increasing the amount of glyceryl triester in the composition. It the drawn yarn is to be further treated by being bulked in a false-twist texturing process, the tension prior to the draw pin should be about 5 to 15 grams. This reduction in tension is related to increased friction between the yarn and the draw pin and is representative of the relationship which must be maintained in a subsequent texturing step wherein twist is removed at the twist trap. If the friction between the yarn and the twist trap is too low, twist can slip through the trap and result in the undesirable appearance of tight spots, i.e., twisted sections, in the bulked yarn. Compositions of this invention providing a tension prior to the draw pin of about 5 to grams give excellent drawing and false-twist texturing performances.

These compositions are easily dispersed to form stable emulsions which do not give rise to gels on evaporation of the water. Yarns carrying these compositions are particularly suited for false-twist texturing wherein the yarns are subjected to temperatures of 200 C. and more. The compositions do not cause the formation of hazardous fumes or filament-breaking thermal residues when passed over heated metal surfaces. The false-twisted yarns produced with these compositions show high levels of bulk and strength retention and no evidence of tight spots.

In the production of bulky yarns from continuous filament yarns, the degree to which the original strength is retained is of the greatest importance. As is known, the normally compact yarn bundle is rearranged by altering the straight filaments by imparting to them bends, loops, whorls, and the like. As a result of this rearrangement, an applied load is no longer borne equally by all of the filaments in the bundle and the yarn strength decreases accordingly. If the yarn is not textured uniformly, some sections of the yarn will contain fewer load bearing filaments and the strength loss will be excessive. It is believed that the compositions of this invention provide a high level of strength retention by functioning in a constant and uniform manner as a lubricant when the set twist of the yarn is being removed at the twist trap, and thus contribute to the formation of uniform bulky yarns. Further, the temperature-related properties of these compositions do not cause strength loss by promoting polymer degradation. Strength retention is determined by measuring the tenacity of the yarn before and after texturing. The percent strength retention is calculated from the formula Percent Strength Retention=100( 100) wherein:

T =Tenacity of prebulked yarn, and T =Tenacity of bulked yarn.

In the following examples, which are given to illustrate the invention further, all parts are by weight and all percentages are by weight based on the total weight of the components.

EXAMPLE I An oily blend is obtained by stirring together parts of the sodium salt of sulfated peanut oil (containing approximately 23% water) and 20 parts of refined coconut oil. A fatty acid salt is prepared by mixing 19 parts of oleic acid, 4 parts of triethanolamine, and 6 parts of potassium hyroxide (as a aqueous solution), and about half of this salt is added to the oily blend. These combined ingredients are then emulsified by stirring them into 630 parts of water.

A mixture is prepared by adding the remainder of the above-described fatty acid salt to 20 parts of the potassium salt of p-octyi phosphate (containing approximately 30% water) consisting of a mixture of esters containing about equal parts of the monoand di-ester. The mixture is stirred into 270 parts of water to form an emulsion which is then added to the previously prepared emulsion to form a final emulsion containing about 10% solids. This emulsion is then roller-applied to a freshly-spun 34-filament polyhexamethylene adipamide yarn.

The yarn, containing 0.50% of the emulsion solids, is then drawn in a conventional manner to a denier of 70. There are 0.006 breaks/lb. and 1.5 filament wraps. Yarn tension just prior to the draw pin is 7 grams.

The yarn is then false-twist textured on a Superloft Model 553 texturing machine. The false-twist spindle rotates at a speed of about 240,000 revolutions per minute and applies about turns per inch of false twist to the yarn. The twist on the feed side of the spindle is set into the yarn by passing the yarn over a metal plate, 27 inches (68.5 centimeters) in length, heated to a temperature of about 230 C. The yarn is untwisted at the twist trap to form a bulky yarn which is wound up at a speed of about 70 yards (64 meters) per minute. No fumes are produced, and the yarn has a high bulk level with no tight spots. The strength retention is 76%.

EXAMPLE II A 10% emulsion is prepared in the manner as described in Example I. The emulsion is prepared from 40 parts of the sodium salt of sulfated peanut oil, 10 parts of coconut oil, 19 parts of oleic acid, 4 parts of triethanolamine, 7 parts of potassium hydroxide (45% aqueous solution) and 20 parts of the potassium n-octyl phosphate of Example I.

Nylon yarn carrying this composition is false-twist textured as described in Example I and gives a bulky yarn having a strength retention of 69%.

EXAMPLE III A 10% emulsion is prepared in the manner described in Example I. The emulsion is prepared from 40 parts of the sodium salt of sulfated peanut oil, parts of coconut oil, 21 parts of oleic acid, 5 parts of triethanol amine, 7 parts of potassium hydroxide (45% aqueous solution) and 22 parts of potassium dioctyl phosphate.

Polyethylene terephthalate yarn carrying this composition is false-twist textured in a manner similar to that described in Example I and gives a bulky yarn with good strength retention.

EXAMPLE IV An oily mixture is prepared by adding together 29.6 parts of the sodium salt of a sulfated peanut oil, 22 parts of coconut oil and 16.4 parts of oleic acid. A portion of the fatty acid salt is then formed by stirring in 4.4 parts of triethanol amine. The mixture is then heated to 50 C. and the remainder of the fatty acid salt formed by the addition of 2.0 parts of potassium hydroxide. The potassium hydroxide addition consists of potassium hydroxide dissolved in enough water to give a concentration of 45%, by weight. There is then added 17.8 parts of a mixture of monoand di-n-octyl phosphate; the two free acid esters being present in a ratio of about one part monoester to one part diester. The temperature is raised to 60 C. with agitation. Agitation is continued until a clear blend is formed and while the composition is allowed to cool to room temperature. The blend is then emulsified by stirring it into caustic water heated to 75 C. The caustic water is prepared by adding 7.2 parts of potassium hydroxide in a 45%, by weight, solution. The emulsion is cooled to 40 C. and 0.48 part of a 37%, by weight, solution of formaldehyde is stirred into the emulsion.

Nylon yarn treated with this composition is false-twist textured as described in Example I and gives a bulky yarn with good strength retention.

EXAMPLE V An oily mixture is prepared by adding together 26.6 parts of the sodium salt of a sulfated peanut oil, 29.4 parts of coconut oil and 14.3 parts of oleic acid. A portion of the fatty acid salt is then formed by stirring in 3.8 parts of triethanol amine. The mixture is then heated to 50 C. and the remainder of the fatty acid salt formed by the addition of 1.4 parts of potassium hydroxide. The potassium hydroxide addition consists of potassium hydroxide dissolved in enough water to give a concentration of 45 by weight. There is then added 16.2 parts of a mixture of monoand di-n-octyl phosphate; the two free acid esters being present in a ratio of about one part monoester to one part diester. The temperature is raised to 60 C. with agitation. Agitation is continued until a clear blend is formed and while the composition is allowed to cool to room temperature. The blend is then emulsified by stirring it into caustic water heated to 80 C. The caustic water is prepared by adding 5.5 parts of potassium hydroxide in a 45%, by weight, solution. The emulsion is cooled to 40 C. and 0.48 part of a 37%, by weight, solution of formaldehyde is stirred into the emulsion.

Nylon yarn treated with this composition is false-twist textured as described in Example I and gives a bulky yarn with good strength retention.

EXAMPLE VI An oily mixture is prepared by adding together 23.8 parts of the sodium salt of a sulfated peanut oil, 37.6 parts of coconut oil and 12.8 parts of oleic acid. A portion of the fatty acid salt is then formed by stirring in 3.3 parts of triethanol amine. The mixture is then heated to 5 0 C. and the remainder of the fatty acid salt formed by the addition of 1.2 parts of potassium hydroxide. The potassium hydroxide addition consists of potassium hydroxide dissolved in enough water to give a concentration of 45%, by weight. There is then added 13.8 parts of a mixture of monoand di-n-octyl phosphate; the two free acid esters being present in a ratio of about one part monoester to one part diester. The temperature is raised to 60 C. with agitation. Agitation is continued until a clear blend is formed and while the composition is allowed to cool to room temperature. The blend is then emulsified by stirring it into caustic water heated to C. The caustic water is prepared by adding 4.9 parts of potassium hydroxide in a 45 by weight, solution. The emulsion is cooled to 40 C. and 0.48 parts of a 37%, by weight, solution of formaldehyde is stirred into the emulsion.

Nylon yarn treated with this composition is false-twist textured as described in Example I and gives a bulky yarn with good strength retention.

From the foregoing discussion and description, it is evident that the present invention is particularly effective in that it permits yarn production at high temperatures and, upon texturing, facilitates the production of yarn with good bulk without material sacrifice in strength. While the invention has been described with respect to specific materials and other details it should be apparent that changes can be made therefrom without departing from its scope.

I claim:

1. Textile yarn comprising filaments of synthetic polymer selected from the group consisting of polyamides and polyesters, the filaments having on their surfaces a composition consisting of 5 to 50 parts by weight of a glyceryl triester selected from the group consisting of coconut oil, peanut oil, corn oil, glyceryl trilaurate, glyceryl tripalmitate, and glyceryl dilaurate-palmitate; 20 to 50 parts by weight of an alkali metal salt of a sulfated glyceryl triester of the group consisting of sulfated glyceryl trioleate, sulfated peanut oil and sulfated olive oil; 10 to 30 parts by weight of a sodium, potassium, ammonium, triethanolamine or morpholine salt of a partial phosphate ester of the group consisting of monoand di-esters of phosphorus pentoxide and an aliphatic alcohol having 6 to 18 carbon atoms per molecule or mixtures thereof; and 10 to 35 parts by weight of an alkali metal, ammonium, or amine salt of a higher fatty acid which contains 12 to 18 carbon atoms per molecule.

2. Textile yarn in accordance with claim 1 in which the yarn contains about 0.1 to 1.5 weight percent of the composition.

3. In the preparation of yarn for false-twist texturing in which polymer of the group consisting of polyamides and polyesters is melt-spun to produce filamentary strands, the strands are coated, collected to a yarn, drawn and then false-twist textured; the improvement comprising coating the filamentary strands before false-twist texturing with a 5 to 30 percent aqueous emulsion of a composition consisting of 5 to 50 parts by weight of a glyceryl triester selected from the group consisting of coconut oil, peanut oil, corn oil, glyceryl trilaurate, glyceryl tripalmitate, and glyceryl dilaurate-palmitate; 20 to 50 parts by weight of an alkali metal salt of a sulfated glyceryl triester of the group consisting of sulfated glyceryl trioleate, sulfated peanut oil and sulfated olive oil; 10 to 30 parts by Weight of a sodium, potassium, ammonium, triethanolamine or morpholine salt of a partial phosphate ester of the group consisting of monoand di-esters of phosphorus pentoxide and an aliphatic alcohol having 6 to 18 carbon atoms per molecule or mixtures thereof; and 10 to 35 parts by weight of an alkali metal, ammonium, or amine salt of a higher fatty acid which contains 12 to 18 carbon atoms per molecule.

4. A composition for application to textile yarn of synthetic polymer selected from the group consisting of polyamides and polyesters, the composition consisting of a 5 to 30 percent aqueous emulsion of a composition of 5 to 50 parts by weight of a glyceryl triester selected from the group consisting of coconut oil, peanut oil, corn oil,

glyceryl trilaurate, glyceryl tripalmitate, and glyceryl dilaurate-palmitate; 20 to 50 parts by Weight of an alkali metal salt of a sulfated glyceryl triester of the group consisting of sulfated glyceryl trioleate, sulfated peanut oil and sulfated olive oil; 10 to 30 parts by weight of a 5 sodium, potassium, ammonium, triethanolamine or morpholine salt of a partial phosphate ester of the group consisting of monoand di-ester of phosphorus pentoxide and aliphatic alcohols having 6 to 18 carbon atoms per molecule or mixtures thereof; and 10 to 35 parts by weight of an alkali metal, ammonium, or amine salt of a higher fatty acid which contains 12 to 18 carbon atoms per molecule.

- References Cited UNITED STATES PATENTS FOREIGN PATENTS 7/1959 Great Britain. 12/ 1917 Great Britain.

10 HERBERT B. GUYNN, Primary Examiner US. Cl. X.R. 

